Preparation method of pirimicarb molecularly imprinted polymer

A molecular imprinting and polymer technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of staying in the evaluation stage of the physical characteristics and adsorption properties of polymers, difficult elution of pirimicarb, etc., and achieve large-scale promotion. Application value, improving detection sensitivity and detection efficiency, and the effect of efficient enrichment

Inactive Publication Date: 2012-12-26
SHANGHAI JIAOTONG UNIV
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Problems solved by technology

[0004] Find through the retrieval of prior art document, the article " Piezoelectric quartz crystal sensor for rapid analysis of pirimicarb residues using molecularly imprinted polymers as recognition elements " (using molecularly imprinted polymers as recognition elements " published on " Analytica Chimica Acta " 2006,576,67-76 by Fung etc. Piezoelectric quartz crystal sensor with imprinted polymer as identification material for rapid detection of pirimicarb residue) synthesized anti-pirimicarb molecularly imprinted polymer; Pingarrón et al. The article "Molecularly imprinted polymers for on-line preconcentration by solid phase extraction of pirimicarb inwater samples" also synthesized pirimicarb molecularly imprinted polymers; However, the polymerization method used in these two papers is an in-situ polymerization method, and there is a problem that it is difficult to elute the pirimicarb bound to the polymer.
Gao et al. published the article "Molecular imprinted material prepared by novel surface imprinting technique for selective adsorption of pirimicarb" in their paper "Polymer" 2008, 49, 1230-1238 (the preparation of anti-pirimicarb by novel surface polymerization technology has selective adsorption Molecularly imprinted polymers) synthesized anti-pirimicarb molecularly imprinted polymers by surface grafting, but this article only stayed at the evaluation stage of polymer physical characteristics and adsorption properties

Method used

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  • Preparation method of pirimicarb molecularly imprinted polymer
  • Preparation method of pirimicarb molecularly imprinted polymer

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Experimental program
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Effect test

Embodiment 1

[0025] Mix 0.2mmol of pirimicarb, 0.8mmol of TFMAA, and 4mmol of EDMA, dissolve in 20mL of heptane, let it stand at room temperature for 2 hours, and then add 0.08mmol of initiator ACPA-silica gel.

[0026] The above mixture was placed in an ampoule, and degassed by ultrasonic vibration for 10 minutes. The degassed system was purged with nitrogen for 5 minutes. Quickly seal under nitrogen protection. 65 ℃ water bath insulation reaction for 30 hours. The reaction product is obtained.

[0027] After the reaction, template molecules were removed by Soxhlet extraction for 12 hours. The extraction reagent is 150ml methanol-water-acetic acid mixture (7:2:1, V / V / V). Finally, the residual acetic acid was washed with methanol to neutrality. The polymer from which the template molecule was removed was dried overnight at 60° C. to obtain a molecularly imprinted polymer resistant to pirimicarb. It was determined experimentally that

[0028] The theoretical adsorption capacity of th...

Embodiment 2

[0030] Mix 0.2mmol of pirimicarb, 0.8mmol of TFMAA, and 4mmol of EDMA, dissolve in 20mL of heptane, let it stand at room temperature for 2 hours, and then add 0.08mmol of initiator ACPA-silica gel.

[0031] The above mixture was placed in an ampoule, and degassed by ultrasonic vibration for 5 minutes. The degassed system was purged with nitrogen for 10 minutes. Quickly seal under nitrogen protection. 70 ℃ water bath insulation reaction for 20 hours. The reaction product is obtained.

[0032] After the reaction, template molecules were removed by Soxhlet extraction for 12 hours. The extraction reagent is 150ml methanol-water-acetic acid mixture (7:2:1, V / V / V). Finally, the residual acetic acid was washed with methanol to neutrality. The polymer from which the template molecule was removed was dried overnight at 60° C. to obtain a molecularly imprinted polymer resistant to pirimicarb. It was determined experimentally that

[0033] The molecularly imprinted polymer prepare...

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Abstract

The invention discloses a preparation method of a pirimicarb molecularly imprinted polymer in the field of biochemical technology, which comprises the following steps: dissolving a template molecule, i.e. pirimicarb, a functional monomer i.e. trifluoromethyl acrylic acid (TFMAA) and a cross-linking agent, i.e. ethylene glycol dimethacrylate (EDMA) into a pore-forming agent according to the molar ratio of template molecule to functional monomer to cross-linking agent of 1:4:20; adding an initiator; carrying out nitrogen protection and then performing a water bath heat preserving reaction; removing the template molecule through Soxhlet extraction; and drying the polymer at 60DEG C overnight after the template molecule is removed to obtain the pirimicarb molecularly imprinted polymer. The invention effectively purifies the matrix, efficiently enriches the pirimicarb, and remarkably improves the detection sensitivity and the detection efficiency of the pirimicarb by being combined with the prior detection methods (HPLC and the like).

Description

technical field [0001] The present invention relates to a preparation method in the field of biochemical technology, in particular to a preparation method of pirimicarb molecularly imprinted polymer (molecularly imprinted polymer, MIP). Background technique [0002] Pirimicarb can control all aphids except cotton aphids that are resistant to organophosphate insecticides, and is often used for the control of aphids in vegetables. The toxic mechanism of carbamate pesticides is mainly to inhibit the activity of cholinesterase, so that the hydroxyl group of serine in the active center of the enzyme is carbamylated, thus losing the ability of the enzyme to hydrolyze acetylcholine. Due to the over-limit and over-range use of pirimicarb, the resulting pressure on the environment and food safety has become increasingly prominent. All countries in the world have made strict regulations on the use and residues of carbamate pesticides and formulated corresponding standards. Among them...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F222/14C08F220/04C08J9/26B01J20/285B01J20/30
Inventor 孙向军唐波陈秋宇
Owner SHANGHAI JIAOTONG UNIV
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